Distillation apparatus.



HARRYO. CHUTE, OF CLEVELAND, OHIO.

DISTILLATION APPARATUS.

"Specification of Letters Patent.

Patented Aug. 18, 1908.

Application filed. December. 3, 1904. Serial No. 235,280.

To all @071 am it may concern:

Be it known that I, HARRY O. CHUTE, a citizen of the United States, anda resident of the city of, Cleveland, county of Cuyahoga,

State of Ohio, have invented certain new and useful Improvements inDistillation Apparatus, of which the following is a full, clear, andexact description.

This invention relates to apparatus of the kind known as continuousstills, and relates particularly to stills employed for the separationof wood alcohol from pyroligneous acid, though of course such stills maybe used for other purposes.

The invention consists in the combination, with a column still, of aseparate boiler or heater of improved construction; in means employedfor avoiding the feeding of ta y or other insoluble matter into thisheate in means for regulating the point of entry into the still of thecrude liquor and the returns from the exchanger; in means for admittingsaid returns at a point above that at which the crude liquor isadmitted; in novel means for testing the quality of the vapor in thestill; and in various other features, as hereinafter more fullydescribed and particularly pointed out in the claims.

The objects of my invention are, to increase the efliciency offractional distilling apparatus, such as may be employed for thedistillation of pyroligneous acid; to avoid the dilution of the liquorWithin the still by steam or like vapor employed for heating; to improvethe means employed for applying heat in the still; to prevent the entryof tarry matter into the heater; to provide improved means forregulating the action of the still; to provide means for. testing atwill the vapors in the still; and generally to make the apparatussimple, durable and highlyeflicient.

I will now proceed to describe my invention with reference to theaccompanying drawings, illustrating diagrammatically one form ofapparatus embodying my invention, and will then point out the novelfeatures in claims. The said drawing shows a side elevation of'theapparatus, parts of which have been broken away or sectioned to show theinternal construction.

In this showing, Figure 1 illustrates the apparatus as a whole, partlyin elevation and partlyin vertical section; and Fig. 2 illustrates, onan'exag erated scale, the connec-' tion of pipes man a of Fi 1.

In my apparatus, I pre erably employ a heatin oontinuousl actingcolumnchambered still of the type nown as beer stills, in which.

the raw or crude liquor fed into the same at or near the top anddescending therethrough is subjected to the action of the ascendingheated vapors produced by vaporizing a selected portion'of the liquorremoved from that remaining after the evaporation of the alcohol. thisselected portion is preferably structurally separate from the still andcomprises upper and lower chambers and an intermediate heating chamber,through which pass heating tubes connecting the upper and lowerchambers, said tubes being heated by live steam or' other heating fluidcirculating around them in said heating chamber. The chamber has nofluid connection with t e liquid chambers. Said boiler further comprisesexterior circulating tubes connecting the upper and lower liquidchambers.

The lower compartment or chamber of the still constitutes a settlingchamber of capacity sufficient to permit the tarry and other insolubleproducts to settle, automatic means being provided for drawing off thesetarry products with the liquor in said chamber and for maintaining asubstantially uniform level of liquid in said chamber. A pipe having anadjustable end piece, is provided for drawing off a portion ofsubstantially tar free or clear li uor from this chamber, and conductingsuc liquor to the boiler before mentioned; and another pipe conducts thevapor from this boiler back into the still. The liquor to be distilledenters the upper portion of the still, after first passing through asuitable heat-exchanger Wherein there is an exchange of heat between theoutgoing vapors from the still and the incoming liquor. By means ofsuitable valves, the incoming liquor may be admitted to the still at anyone of a plurality of chambers of said still; and by similar means thevapors condensed in the exchanger, may be returned to the still at anyone of a plurality of points. Preferably inflowing liquid is introducedat a point in the still Where the average alcoholic richness of theliquid on the plates in the chamber is not widely different from that ofsuch inflowingliquid. In connection with the still, I preferably employwhat I term a tester consisting of a small condenser arranged to beconnected at will, to

The boiler used for so vaporizing any one of a number of thelowerchambers of the still, and to draw off vapors from the large proportionof the liquor.

particular chamber with which it may be connected at any moment. Vaporsso drawn off and Condensed, flow into a suitable hydrometer cup, whereinfloats a hydrometer. By this means, the quality of the vapors in thevarious chambers of the still connected to the tester, may be determinedreadily whenever desired.

Pyroligneous liquor is the aqueous portion of the products from thedestructive distillation of wood. It contains besides a large uantity ofwater, methyl 'alcohol which oils at 66 degrees centigrade,, andacetoneboiling at 56 degrees centigrade, which two latter materialstogether for the wood alcohol of commerce. Pyroligneous liquor alsocontains acetic acid-boiling at 119 degrees centigrade, and otherorganic volatile acids, and the liquor also contains more or less tarryproducts. In distilling such liquor with the apparatus ordinarily used,the alcohol, if completely distilled off from the liquor, carries withit a portion of' the acids; and to so distil ofl practically all of thealcohol requires the evaporation of a My apparatus serves to separatethe alcoholic or spirituous portion of the liquid in a concentratedstate, substantially free from acid and delivers the acid portionundiluted, no free steam being used in heating.

Referring now to the drawing, a designates an ordinary column still. Ido not illustrate the'same in detail, as the construction of such stillsis well understood. It will be understood that such still comprises aplurality of chambers through which the liquor treated descendsrogressively, and through which the heated vapor ascends progressively.At the base of' this still there 1s a settling chamber b. Adjacent tothe still is a heater or boiler p comprising upper and lower chambers 9and w respective and an intermediate heating chamber t, which latterchamber is steam-tight and contains a large number of ubes 8 connectingchambers g and w. Steam or other suitable heating fluid may be ad ittedto this chamber t through a connegtion u, and the exhaust or condensedsteam, or heating fluid, esca es through a connection '0. Chambers g anw are further connected by external clrcul'ating ipes r.

Pipes 1' being air-cooled cause a circu ation of liquid downwardtherethrough.

ll The heater or boiler thus constructed may e made quite cheaply, andthe tubejs s,

which are exposed to the steam pressure,

may be made quite small, thus permitting them to withstand relativelyhigh steam pressure even when made of relatively thin weak material.

The liquor to be distilled is passed by suitable means, such as a pump Zand pi e is, into an exchan er i of famillar form s own in section, anthence passes through a trapped pipe it into the column a.

Said ipe h is connected with the column at a plura ity of points bymeans of valves h, h and h The vapor from the column passes through thepipef into the heating chamber of the exchanger i and thence passes intothe main condenser j, and when condensed, out through pipe at. Any vaporwhich may be condensed in the exchanger may be returned to the stillthrough a trapped pipe g connected with the column at a plurality ofpoints, by means of valves 9 g g and g Thev settling chamber b at thebottom of the still, is provided with a pi e e, the mouth of which isnear the bottom 0 such chamber, through which pi e the tarry products,

hich settle to the ottom of this chamber 1), a the acid liquor may bedrawn off. Float 0, operating a valve d in said ipe, regulates the evelof the liquid in cham er b. A pipe n opening into the chamber at a pointabove the level of the draw-off pipe e, serves to draw ofl a portion ofthe liquor substantially free from tar or other insoluble .im uritiesand also free from alcohol and the li e from chamber b and to introducethe same into the boiler and, as shown, this pipe has an adjustablemouth piece m, whereby the level of the inlet mouth of this pipe, may bevaried. In the construction shown, this mouth iece m is a sim le benttube, by turning wiich, the level 0? the mouth may be adjusted asdesired. The vapors are. returned from the boiler 19 to the u per ortionof chamber 6, above the level 0 the liquid therein, through a pipe 0.100

As shown in Fig. 2, pipe at is provid d with a screw union consisting ofa flange 2 the outside of which is threaded and rigidl attached to thepipe m, a flange 23 rigidly attached to pipe n, and collar 21 fittingoer flange 23 and screwing on to the thread n flange 22. This permitspipe m to be turnel relative to pipe n and therefore permits th mouth ofpi e m to be adjusted relative to the liquid evel in the settlingchamber. Any other type of rotatable union however may of course be usedand the type shown is,;. merely exemplificatory.

The operation of this apparatus is as fol: lows: The crude liquorentering through pipe is, is heated prelinunarily, during its passage lthrough the exchanger 01, and thence passes into the still through pipeh and one or another, or two or more of the valves h h and h Within thestill, it descends successively from chamber to chamber of the still,being heated therein by the ascending vapors, the alcohol within theliquor being thereby distilled ofl fractionally and caused to pass oflthrough pipe f, while aqueous vapor, acid vapor and the like, in theuprising vapors, are condensed and caused to descend. The liquor whichcollects in chamber b is substantially free from alcohol, and any tartherein collects in the lower portion of said 15:0

' the level of liquid in the chamber disturbance of the liquor in thechamber being prevented by introducing inflowing liquid near its bottomthrough pipe 'y and is drawn off through pipe 6, together with the acid.A portion of the substantially tar-free liquid from the top layers ofthe mass of liquid within such chamber 1) is drawn off through pipe nand passed through the heater or boiler 19, whereby such liquor isevaporated and its vapor returned through pipe 0 tothe still, suchvapors rising through the chambers of the still and constituting themeans whereby the alcohol is distilled off from the descending liquid.Both a and 0, in the structure shown, being freely open settlingchamber 1) and boiling chamber 1) will be the same. The valves h, if,and h permit the entering liquors to be admitted to the still atdiflerent heights in order that substantially all of the alcohol shallbe evaporated. The various valves g g g and g permit the condensationfrom exchanger 0', to bereturned to the still at various points. Suchcondensation liquors, being exceedingly rich in alcohol, serve tocondense any acid remaining in the vapors after its passage through thecrude entering liquor, without depriving the uprising va pors of theiralcohol. In order that this finalseparation may be efficient, Ipreferably so adjust the valves mentioned, that the crude liquor entersthe still below the condensation liquor returned from the exchanger i.By properly adjusting these various valves, the operation of the stillmay be so regulated as to regulate the percentage. of the alcohol in thedistillate while completely separating the alcohol from the acid, all inone operation.

I By use of the separate heater p I avoid the introduction of steam intothe still, as has been done heretofore; the introduction of steam beingobjectionable ordinarily because it tends to dilute the acid liquor andrender the separation more expensive. However, if desired, as forheating the apparatus in starting steam may be admitted through theopening 3. By means of theadjustable mouth piece m, I avoid drawing intothe boiler, not merely the main mass of tar which collects at the bottomof the chamber 5, but even the separateglobules of tar which have not asyet coalesced. In this way I avoid the baking of the tar on the surfacesof the heating tubes of the boiler 1), which, ifit occurs, materiallylowers the efficiency of the heater.

In order to be able to test the liquor in the still and determine thequality of the liquor in the various lower chambers, I employ a tester2, comprising a small condenser connected to the lower portion of thestill at various points, by means of a pipe 4 and valves 5, suchcondenser being provided with an inlet 6 and outlet 7 for cooling fluid.

The vapors drawn through pipe 4 into this condenser, drop through pipe 9into hydrometer cup 8. The hydrometer serves to indicate the averagerichness of the vapors in the chambers with which the tester is placedin communication. By this means may be determinedthe point in the stillat which the liquor becomes substantially free of alcohol.

In the drawing, 1 designates a pressure gage of familiar form,comprising a cylinder connected at its upper end to the still and a pipeextending upward from such cylinder; which pipe is customarily providedwith in dicating means at a point above that at which the pipe is shownas broken oil in the drawing.

The still is supported on a base 23, which may be of any desired shapeor construction.

What I claim is; I

1. In distillation apparatus, the combination with a chambered columnstill provided at its lower end with a quieting and settling chamber andwith a draw-oil outlet, of a heater having a liquid supply passagecommunicating with said settling chamber at a point above said outlet,said heater provided with lneans for returning vapor to said settlingchamber near the top thereof 2. In distillation apparatus, the ml)lll21tion with a chambered column still provided.

at its lower end with a settling chamber and I with a draw-ofl outlet,and automatic levelregulatin'g means controlling such outlet, of aheater having a supply passage communicating with said settling chamberat a point above said outlet, said heater provided with a connection forreturning vapor to said still.

3. In distillation apparatus, the combination with a chambered columnstill provided at its lower end with a settling chamber and with adraw-off outlet, of a heater having a liquid supply passagecommunicating with such settling chamber, and provided with means foradjusting the point of communication. to various heights above saidoutlet, said heater further provided with means for returning vapor tothe still.

4. In distillation apparatus, the combination with a chambered columnstill provided at its lower end with a settling chamber and with adraw-oii outlet, and automatic levelregulating means controlling suchoutlet,-

of a heater having a supply passage communicating with such settlingchamber and provided with means for adjusting the point of communicationto various heights above said outlet, said heater further provided withmeans for returning vapor to the still.

5. In distillation apparatus, the combination with a chambered columnstill provided at its lower end with a settling chamber, of a heater andmeans connecting the same with said settling chamber comprising a bentpipe Within such chamber rotatable to vary the level of its mouth, saidheater provided with-means for returning vapor to the still.

6. In distillation apparatus, the combination with a chambered columnstill having a quieting and settling chamber at its base,

. of a separate heater therefor comprising up- Ipier and lower chambers,an intermediate eating chamber, pipes passing through such tion with achambered column still provided with heating means, of an exchangertherefor, provided with vapor and liquor connections comprisingadjustable means for admitting the heated liquor to said still at anyone of a plurality of levels, and comprising also means for returningcondensed liquid to said still at any one of a plurality of levels.

8. Indistillation apparatus, the combination with a continuously fedchambered column still comprising heating means and means for supplyingliquor to the upper portion thereof and means for withdrawing exhaustedliquor from the base, of a tester comprising a condenser provided withmeans for connecting it to the vapor spaces of the still at any one of aplurality of intermediate levels to draw ofi vapor, and comprising alsomeans for indicating the quality of the liquid condensed from the vaporso drawn off.

9. In distillation-apparatus, the combination With a continuouslyoperating chambered column still comprising heating means and means forsupplying liquor to the upper portion "thereof and means for withdrawingexhausted liquor from the base, of a tester comprising a condenserprovided with means for'connecting it to the vapor spaces of the stillat any one of a plurality of intermediate levels to draw ofi vapor, areceptacle receiving the fluid condensed, and a hydrometer therein.

'10. In distillation apparatus, a continu- .ously operatingfractionating still comprising a chambered column still, means forcontinuously feeding raw hot liquor into an upper chamber thereof,'saidmeans com- .i risin a heat exchanger adapted to transfer eat omoutfiowing vapors to inflowing liquor, a quieting and settling chambercommunicating with the column still at the base thereof and providedwith automatically actin means for preserving a constant liqui leveltherein by drawing oif regulated amounts of liquid from the base of saidquieting chamber, and a heating chamber arranged to take liquid fromsaid settling chamber at a point above the automatically controlledliquid outlet thereof and to return vapors of said liquid to a pointnear the top of said settling chamber and above the normal liquid leveltherein.

In testimony whereof I aflix my signature in presence of two witnesses.

HARRY O. GHUTE. [L. s.]

Witnesses:

T. M. KREGELIUS, H. L. PAYNE.

